Login In
2016 Volume 32 Issue 2
2016, 32(2): 193-201
doi: 10.11862/CJIC.2016.004
Abstract:
Ce0.65Zr0.35O2 (CZ) was synthesized by soft-hard template method and its corresponding Pd only catalyst was also prepared. The intermediate product and CZ were characterized by energy dispersive spectrometer (EDS) and laser raman spectroscopy. The Pd/CZ catalyst was investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2-physical adsorption, oxygen storage capacity (OSC), impulse CO chemisorption and H2-temperature programmed reduction (H2-TPR) technologies. It was found that soft-hard template method offered catalyst with high surface area and pore volume, enhanced the ratio of Ce3+, Pd dispersion and homogeneity of solid solution. It also imparted catalyst excellent three-way catalytic performance before and after aging. After aging, the light-off temperatures to C3H8, CO and NO were 318, 180 and 210 ℃ respectively, which were lower than aged catalyst synthesised by soft template, behaved strong anti-sintering property.
Ce0.65Zr0.35O2 (CZ) was synthesized by soft-hard template method and its corresponding Pd only catalyst was also prepared. The intermediate product and CZ were characterized by energy dispersive spectrometer (EDS) and laser raman spectroscopy. The Pd/CZ catalyst was investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), N2-physical adsorption, oxygen storage capacity (OSC), impulse CO chemisorption and H2-temperature programmed reduction (H2-TPR) technologies. It was found that soft-hard template method offered catalyst with high surface area and pore volume, enhanced the ratio of Ce3+, Pd dispersion and homogeneity of solid solution. It also imparted catalyst excellent three-way catalytic performance before and after aging. After aging, the light-off temperatures to C3H8, CO and NO were 318, 180 and 210 ℃ respectively, which were lower than aged catalyst synthesised by soft template, behaved strong anti-sintering property.
2016, 32(2): 202-210
doi: 10.11862/CJIC.2016.019
Abstract:
A nano-sized Ru-Zn catalyst was prepared by a co-precipitation method and the effect of arabic gum modification on the performance of Ru-Zn catalysts was investigated. The catalysts were characterized by X-ray diffraction (XRD), transimission electron microscopy (TEM), N2 physisorption, X-ray photoelectron spectroscopy (XPS), and X-ray fluorescence (XRF). It was found that the dosage of arabic gum could tune the particle size of the Ru-Zn catalysts. The maximum cyclohexene yield showed a volcanic-type variation tendency with the particle size of Ru-Zn catalysts increasing. When the mass ratio of arabic gum to RuCl3·xH2O was 0.033, a Ru-Zn catalyst with a optimum particle size of 4.0 nm was obtained, and a maximum cyclohexene yield of 59.6% was achieved. Moreover, the catalyst exhibited the excellent reusability.
A nano-sized Ru-Zn catalyst was prepared by a co-precipitation method and the effect of arabic gum modification on the performance of Ru-Zn catalysts was investigated. The catalysts were characterized by X-ray diffraction (XRD), transimission electron microscopy (TEM), N2 physisorption, X-ray photoelectron spectroscopy (XPS), and X-ray fluorescence (XRF). It was found that the dosage of arabic gum could tune the particle size of the Ru-Zn catalysts. The maximum cyclohexene yield showed a volcanic-type variation tendency with the particle size of Ru-Zn catalysts increasing. When the mass ratio of arabic gum to RuCl3·xH2O was 0.033, a Ru-Zn catalyst with a optimum particle size of 4.0 nm was obtained, and a maximum cyclohexene yield of 59.6% was achieved. Moreover, the catalyst exhibited the excellent reusability.
2016, 32(2): 211-215
doi: 10.11862/CJIC.2016.050
Abstract:
The extraction of uranium from high level liquid waste is important. In this paper, a series of structural related asymmetric amide extractant bearing methyl on N atom, such as N-methyl-N-decyloctanamide (MDOA), N-methyl-N-decyl-decanamide (MDDA) and N-methyl-N-decyldodecanamide (MDDOA) was designed and synthesized. The extraction thermodynamics of U (Ⅵ) from nitric acid solutions with the aforementioned extractants in n-octane was investigated in detail and the various factors affected extraction properties were studied.
The extraction of uranium from high level liquid waste is important. In this paper, a series of structural related asymmetric amide extractant bearing methyl on N atom, such as N-methyl-N-decyloctanamide (MDOA), N-methyl-N-decyl-decanamide (MDDA) and N-methyl-N-decyldodecanamide (MDDOA) was designed and synthesized. The extraction thermodynamics of U (Ⅵ) from nitric acid solutions with the aforementioned extractants in n-octane was investigated in detail and the various factors affected extraction properties were studied.
2016, 32(2): 216-222
doi: 10.11862/CJIC.2016.030
Abstract:
Ag3PO4 visible light photocatalyst was prepared by one step precipitation method from silver nitrate and sodium phosphate. It was loaded onto stainless steel mesh support using silica sol, then the photocatalytic electrode was obtained after drying. Using supported photocatalytic electrode and carbon rod as the cathode and the anode respectively, filling granular carbon already loaded with electrogenic microbes in anode chamber, and the coupled photocatalytic microbial fuel cell reactor was established. With RhB as a model pollutant, the effects of light intensity, substrate concentration, pH value on removal efficiency and the electricity generation were studied. The results showed: using 100 W halogen light, a 500 Ω external resistance, at pH=10, and 1.5 times microbial biomass, after 4 h reaction, 92% RhB in 200 mL 50 mgL-1 solution was removed; at this time the output voltage and the power densities were respectively 124 mV and 34.9 mW·m-2. The supported photocatalytic electrode is stable after five times reuses.
Ag3PO4 visible light photocatalyst was prepared by one step precipitation method from silver nitrate and sodium phosphate. It was loaded onto stainless steel mesh support using silica sol, then the photocatalytic electrode was obtained after drying. Using supported photocatalytic electrode and carbon rod as the cathode and the anode respectively, filling granular carbon already loaded with electrogenic microbes in anode chamber, and the coupled photocatalytic microbial fuel cell reactor was established. With RhB as a model pollutant, the effects of light intensity, substrate concentration, pH value on removal efficiency and the electricity generation were studied. The results showed: using 100 W halogen light, a 500 Ω external resistance, at pH=10, and 1.5 times microbial biomass, after 4 h reaction, 92% RhB in 200 mL 50 mgL-1 solution was removed; at this time the output voltage and the power densities were respectively 124 mV and 34.9 mW·m-2. The supported photocatalytic electrode is stable after five times reuses.
2016, 32(2): 223-232
doi: 10.11862/CJIC.2016.045
Abstract:
Ti3+ self-doped TiO2(A)/TiO2(R)/In2O3 nanoheterojunctions were synthesized by hydrothermal treatment of the precursor obtained using TiCl3 and InCl3 as the Ti and In source without the exist of reductant. The effects of hydrothermal treatment temperature on the properties of the samples were studied. The structure, crystallinity, morphology, chemical state and optical properties of the obtained samples were characterized by X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. Rhodamine B (RhB) and phenol solutions were used as simulated wastewater to evaluate the visible-light photocatalytic activity of the nanoheterojunctions. The Ti3+ self-doped TiO2(A)/TiO2(R)/In2O3 nanoheterojunctions exhibited extended visible light absorption and higher photocatalytic activity than that of pure TiO2, In2O3 and Ti3+ self-doped TiO2. The sample obtained after hydrothermal treatment at 200 ℃ for 24 h exhibited the best visible light photocatalytic activity with a reaction rate constant of 0.044 4 min-1, 17.76 and 8.71 times than that of pure TiO2 and In2O3. Photocurrent density results indicated that the improved visible-light photocatalytic properties which could be attributed to the enhanced photogenerated charge separation of the nanoheterojunction.
Ti3+ self-doped TiO2(A)/TiO2(R)/In2O3 nanoheterojunctions were synthesized by hydrothermal treatment of the precursor obtained using TiCl3 and InCl3 as the Ti and In source without the exist of reductant. The effects of hydrothermal treatment temperature on the properties of the samples were studied. The structure, crystallinity, morphology, chemical state and optical properties of the obtained samples were characterized by X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-Vis diffuse reflectance spectroscopy. Rhodamine B (RhB) and phenol solutions were used as simulated wastewater to evaluate the visible-light photocatalytic activity of the nanoheterojunctions. The Ti3+ self-doped TiO2(A)/TiO2(R)/In2O3 nanoheterojunctions exhibited extended visible light absorption and higher photocatalytic activity than that of pure TiO2, In2O3 and Ti3+ self-doped TiO2. The sample obtained after hydrothermal treatment at 200 ℃ for 24 h exhibited the best visible light photocatalytic activity with a reaction rate constant of 0.044 4 min-1, 17.76 and 8.71 times than that of pure TiO2 and In2O3. Photocurrent density results indicated that the improved visible-light photocatalytic properties which could be attributed to the enhanced photogenerated charge separation of the nanoheterojunction.
2016, 32(2): 241-249
doi: 10.11862/CJIC.2016.041
Abstract:
The spherical and flower-like ZnO nanostructures have been synthesized by a simple hydrothermal reaction of Zn (NO3)2·6H2O with NH3·H2O by varying the volume ratio of ethylene glycol and water at 140 ℃ for 2 h, respectively. The products were characterized by SEM, XRD, UV-Vis DRS and PL, the results showed that the products were single crystalline with the wurtzite structure. The diameter of spherical ZnO nanostructure assembled nanoparticles is ranged from 500 nm~1 μm. The flower-like ZnO nanostructures are assembled from one-dimensional nanorods with the diameter is ranged from 100~300 nm and length is ranged from 300~700 nm. The influence of ethylene glycol on the morphology development was investigated. Possible growth mechanisms of the spherical and flower-like ZnO nanostructures were proposed. Photocatalytic activities of the spherical and flower-like ZnO nanostructures in the degradation of methyl orange were investigated. The degradation rate of the spherical and flower-like ZnO nanostructures under 2 h UV irradiation were 83% and 55%, respectively. The study on photocatalytic mechanism confirmed that h+ and ·OH were the main reactive species during the photocatalytic process.
The spherical and flower-like ZnO nanostructures have been synthesized by a simple hydrothermal reaction of Zn (NO3)2·6H2O with NH3·H2O by varying the volume ratio of ethylene glycol and water at 140 ℃ for 2 h, respectively. The products were characterized by SEM, XRD, UV-Vis DRS and PL, the results showed that the products were single crystalline with the wurtzite structure. The diameter of spherical ZnO nanostructure assembled nanoparticles is ranged from 500 nm~1 μm. The flower-like ZnO nanostructures are assembled from one-dimensional nanorods with the diameter is ranged from 100~300 nm and length is ranged from 300~700 nm. The influence of ethylene glycol on the morphology development was investigated. Possible growth mechanisms of the spherical and flower-like ZnO nanostructures were proposed. Photocatalytic activities of the spherical and flower-like ZnO nanostructures in the degradation of methyl orange were investigated. The degradation rate of the spherical and flower-like ZnO nanostructures under 2 h UV irradiation were 83% and 55%, respectively. The study on photocatalytic mechanism confirmed that h+ and ·OH were the main reactive species during the photocatalytic process.
2016, 32(2): 250-258
doi: 10.11862/CJIC.2016.037
Abstract:
2-furancarbaldehyde-4-hydroxy-benzoylhydrazone (H2L) was synthesized from 4-hydroxybenzoylhydrazine and 2-furancarbaldehyde, and its Cu (Ⅱ) coordination polymer [Cu (HL)2]·2H2O (1) also was prepared. H2L and 1 were characterized by elemental analysis and single crystal X-ray diffraction analysis. The crystal structural analyses show that the crystal of H2L belongs to orthorhombic system space group Pna21, and the crystal of 1 crystallizes in monoclinic system space group P21/c. Thermal gravity analyses were used to investigate the thermal stabilities of H2L and 1, and their apparent activation energy of the decompositions were also calculated. It was found that both of the complex and the ligand possessed higher thermal stability. The binding modes of H2L and 1 with CT-DNA were studied by UV-Vis absorption, and their interaction enthalpies were measured by microcalorimetry. The results showed that the interaction of H2L and 1 with CT-DNA belonged to partial intercalation mode and 1 presented stronger interaction with CT-DNA than H2L. CCDC: 1030242, H2L; 1401955, 1.
2-furancarbaldehyde-4-hydroxy-benzoylhydrazone (H2L) was synthesized from 4-hydroxybenzoylhydrazine and 2-furancarbaldehyde, and its Cu (Ⅱ) coordination polymer [Cu (HL)2]·2H2O (1) also was prepared. H2L and 1 were characterized by elemental analysis and single crystal X-ray diffraction analysis. The crystal structural analyses show that the crystal of H2L belongs to orthorhombic system space group Pna21, and the crystal of 1 crystallizes in monoclinic system space group P21/c. Thermal gravity analyses were used to investigate the thermal stabilities of H2L and 1, and their apparent activation energy of the decompositions were also calculated. It was found that both of the complex and the ligand possessed higher thermal stability. The binding modes of H2L and 1 with CT-DNA were studied by UV-Vis absorption, and their interaction enthalpies were measured by microcalorimetry. The results showed that the interaction of H2L and 1 with CT-DNA belonged to partial intercalation mode and 1 presented stronger interaction with CT-DNA than H2L. CCDC: 1030242, H2L; 1401955, 1.
2016, 32(2): 259-266
doi: 10.11862/CJIC.2016.049
Abstract:
Two new cadmium coordination polymers, {[Cd2(bptc)(H2O)3]·H2O}n (1) and {[Cd2(bptc)(bpp)·H2O]·2.25H2O}n (2), were synthesized under hydrothermal reactions by using biphenyl-2, 4, 4′, 6-tetracarboxylic acid (H4bptc), CdCl2·2.5H2O and 1, 3-di (4-pyridyl) propane (bpp). Both of them were characterized by elemental analysis, IR spectra, single crystal X-ray diffraction. Complex 1 is a binuclear structure with two six-coordinated Cd (Ⅱ), both of which are distorted octahedral structures. The binuclear of Complex 2 is different. One Cd (Ⅱ) is distorted octahedral, and the other is seven-coordinated to form a pentagonal bipyramid. The interaction between two complexes, ligand and DNA was studied by EtBr fluorescence probe. Photoluminescence studies revealed that the interaction of complex 2 to the DNA is stronger than complex 1. CCDC: 952960, 1; 952962, 2.
Two new cadmium coordination polymers, {[Cd2(bptc)(H2O)3]·H2O}n (1) and {[Cd2(bptc)(bpp)·H2O]·2.25H2O}n (2), were synthesized under hydrothermal reactions by using biphenyl-2, 4, 4′, 6-tetracarboxylic acid (H4bptc), CdCl2·2.5H2O and 1, 3-di (4-pyridyl) propane (bpp). Both of them were characterized by elemental analysis, IR spectra, single crystal X-ray diffraction. Complex 1 is a binuclear structure with two six-coordinated Cd (Ⅱ), both of which are distorted octahedral structures. The binuclear of Complex 2 is different. One Cd (Ⅱ) is distorted octahedral, and the other is seven-coordinated to form a pentagonal bipyramid. The interaction between two complexes, ligand and DNA was studied by EtBr fluorescence probe. Photoluminescence studies revealed that the interaction of complex 2 to the DNA is stronger than complex 1. CCDC: 952960, 1; 952962, 2.
2016, 32(2): 267-274
doi: 10.11862/CJIC.2016.036
Abstract:
Through using Wells-Dawson type anion [As2W18O62]6-, CuCl2·2H2O and 5-(4-pyridyl)-1H-tetrazole (4-ptz), two different POM-based compounds containing tri-nuclear copper clusters were synthesized in one-pot under hydrothermal conditions, namely [Cu3(4-ptz)4(H2O)7(As2W18O62)]·42H2O (1) and [Cu3(4-ptz)5(H2O)5(As2W18O62)]·47H2O (2). When we used another Wells-Dawson anion [P2W18O62]6-, CuCl2·2H2O and 5-(3-pyridyl)-1H-tetrazole (3-ptz), another POM-based tri-nuclear copper cluster was also obtained, namely [Cu3(3-ptz)4(H2O)8(P2W18O62)]·33H2O (3). Single crystal X-ray diffraction shows that compound 1 is a tri-nuclear copper cluster supporting pendent structure, and compound 2 is a one dimensional chain with anions and tri-nuclear copper clusters arranging alternately, while compound 3 is a discrete structure containing anions and tri-nuclear copper clusters. 3-ptz and 4-ptz are important structural factors for constructing tri-nuclear copper clusters in compounds 1~3. The electrochemical and photocatalytic activities of the title compounds have been studied. CCDC: 1416806, 1; 1406807, 2; 1406808, 3.
Through using Wells-Dawson type anion [As2W18O62]6-, CuCl2·2H2O and 5-(4-pyridyl)-1H-tetrazole (4-ptz), two different POM-based compounds containing tri-nuclear copper clusters were synthesized in one-pot under hydrothermal conditions, namely [Cu3(4-ptz)4(H2O)7(As2W18O62)]·42H2O (1) and [Cu3(4-ptz)5(H2O)5(As2W18O62)]·47H2O (2). When we used another Wells-Dawson anion [P2W18O62]6-, CuCl2·2H2O and 5-(3-pyridyl)-1H-tetrazole (3-ptz), another POM-based tri-nuclear copper cluster was also obtained, namely [Cu3(3-ptz)4(H2O)8(P2W18O62)]·33H2O (3). Single crystal X-ray diffraction shows that compound 1 is a tri-nuclear copper cluster supporting pendent structure, and compound 2 is a one dimensional chain with anions and tri-nuclear copper clusters arranging alternately, while compound 3 is a discrete structure containing anions and tri-nuclear copper clusters. 3-ptz and 4-ptz are important structural factors for constructing tri-nuclear copper clusters in compounds 1~3. The electrochemical and photocatalytic activities of the title compounds have been studied. CCDC: 1416806, 1; 1406807, 2; 1406808, 3.
2016, 32(2): 275-279
doi: 10.11862/CJIC.2016.035
Abstract:
Two new coordination polymers, {[Cd (L)(EG)0.5(H2O)(SO4)]·EG·H2O}n (1) and [Cd (L)(EG)(SO4)]n (2) (EG=ethylene glycol), were solvothermally synthesized by reactions of flexible imidazole-containing ligand 1, 3, 5-tris (imidazoL-1-ylmethyl) benzene (L) with cadmium sulfate under different reaction conditions. The complexes were characterized by elemental analysis, IR and single crystal X-ray diffraction. Ligand L links Cd (Ⅱ) to form 1D chain in 1 while in 2 the ligand L coordinates with Cd (Ⅱ) to give 2D network, which is further connected by sulfate anions to generate 3D structure. Interestingly, each EG connects two intra-chain Cd (Ⅱ) atoms in 1 and acts as terminal ligand in 2. The sulfate anion acts as terminal ligand in 1 and bridging one in 2. The fluorescence properties of the complexes was investigated. CCDC: 1430130, 1; 1430131, 2.
Two new coordination polymers, {[Cd (L)(EG)0.5(H2O)(SO4)]·EG·H2O}n (1) and [Cd (L)(EG)(SO4)]n (2) (EG=ethylene glycol), were solvothermally synthesized by reactions of flexible imidazole-containing ligand 1, 3, 5-tris (imidazoL-1-ylmethyl) benzene (L) with cadmium sulfate under different reaction conditions. The complexes were characterized by elemental analysis, IR and single crystal X-ray diffraction. Ligand L links Cd (Ⅱ) to form 1D chain in 1 while in 2 the ligand L coordinates with Cd (Ⅱ) to give 2D network, which is further connected by sulfate anions to generate 3D structure. Interestingly, each EG connects two intra-chain Cd (Ⅱ) atoms in 1 and acts as terminal ligand in 2. The sulfate anion acts as terminal ligand in 1 and bridging one in 2. The fluorescence properties of the complexes was investigated. CCDC: 1430130, 1; 1430131, 2.
2016, 32(2): 280-288
doi: 10.11862/CJIC.2016.046
Abstract:
Two 2D heterometallic 4d-4f coordination polymers, {[EuAg (tbc)3 (H2O)]ClO4·H2O}n (1) and {[Eu2Ag3(tbc)6(NO3)2(H2O)2](ClO4)2·2H2O}n (2) (Htbc=4-(1H-1, 2, 4-triazoL-1-yl) benzoic acid) were synthesized under hydro-thermal condition using one-step approach and structurally characterized by elemental analysis, FT-IR, powder X-ray diffraction and single-crystal X-ray diffraction. The single-crystal X-ray diffraction analysis reveals that the two complexes present two different types of two dimensional (2D) structures. Complex 1 crystallized in an orthorhombic manner having a P212121 space group, consisting of 1D triple-stranded helical (PPM) [Eu (μ3-OCO)2 (μ2-OCO)] motif as chain which are further linked by the fragments of tbc-ligands and Ag (Ⅰ). Polymer 2 is crystallized in a triclinic fashion having a P1 space group, consisting of 1D mesomeric chains [Eu (μ3-OCO)2] which were further linked by the two different [N-Ag-N] units to form an interesting 2D 4d-4f heterometallic coordination polymer in the ab plane. The solid-state luminescent behaviors of compounds 1 and 2 were investigated at room temperature. CCDC: 1018336, 1; 1024087 2.
Two 2D heterometallic 4d-4f coordination polymers, {[EuAg (tbc)3 (H2O)]ClO4·H2O}n (1) and {[Eu2Ag3(tbc)6(NO3)2(H2O)2](ClO4)2·2H2O}n (2) (Htbc=4-(1H-1, 2, 4-triazoL-1-yl) benzoic acid) were synthesized under hydro-thermal condition using one-step approach and structurally characterized by elemental analysis, FT-IR, powder X-ray diffraction and single-crystal X-ray diffraction. The single-crystal X-ray diffraction analysis reveals that the two complexes present two different types of two dimensional (2D) structures. Complex 1 crystallized in an orthorhombic manner having a P212121 space group, consisting of 1D triple-stranded helical (PPM) [Eu (μ3-OCO)2 (μ2-OCO)] motif as chain which are further linked by the fragments of tbc-ligands and Ag (Ⅰ). Polymer 2 is crystallized in a triclinic fashion having a P1 space group, consisting of 1D mesomeric chains [Eu (μ3-OCO)2] which were further linked by the two different [N-Ag-N] units to form an interesting 2D 4d-4f heterometallic coordination polymer in the ab plane. The solid-state luminescent behaviors of compounds 1 and 2 were investigated at room temperature. CCDC: 1018336, 1; 1024087 2.
2016, 32(2): 289-296
doi: 10.11862/CJIC.2016.038
Abstract:
Simple methods are introduced to obtain hydroxyapatite (HAP, Ca10(PO4)6(OH)2) nanocrystals with different structures and morphologies at mild conditions. The precipitation-hydrolysis two-step method can produce CaHPO4 precursor by assistance of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP) during the precipitation step, and the hydrolysis of CaHPO4 at 100 ℃ under atmospheric pressure leads to the formation of highly crystalline rod-like HAP nanocrystals. The HAP nanorods prepared with PEG possess uniform morphology with high aspect ratio while those prepared with PVP have smaller size with broader size distribution. One-step precipitation method can produce HAP directly, and the nanocrystals prepared with PEG are like wheat ears, while those prepared with PVP were composed of small nanoparticles and nanorods. The morphology of HAP samples was influenced by the organic additives, because the surfactants stabilized and confined the formation and growth of HAP nanocrystals. The morphology and structure of HAP nanoparticles changed greatly via the difference synthetic methods. Therefore, the controlling synthesis of HAP can be achieved by the change of synthetic conditions. The obtained HAP nanoparticles will be applicable for the future biomedical applications.
Simple methods are introduced to obtain hydroxyapatite (HAP, Ca10(PO4)6(OH)2) nanocrystals with different structures and morphologies at mild conditions. The precipitation-hydrolysis two-step method can produce CaHPO4 precursor by assistance of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP) during the precipitation step, and the hydrolysis of CaHPO4 at 100 ℃ under atmospheric pressure leads to the formation of highly crystalline rod-like HAP nanocrystals. The HAP nanorods prepared with PEG possess uniform morphology with high aspect ratio while those prepared with PVP have smaller size with broader size distribution. One-step precipitation method can produce HAP directly, and the nanocrystals prepared with PEG are like wheat ears, while those prepared with PVP were composed of small nanoparticles and nanorods. The morphology of HAP samples was influenced by the organic additives, because the surfactants stabilized and confined the formation and growth of HAP nanocrystals. The morphology and structure of HAP nanoparticles changed greatly via the difference synthetic methods. Therefore, the controlling synthesis of HAP can be achieved by the change of synthetic conditions. The obtained HAP nanoparticles will be applicable for the future biomedical applications.
2016, 32(2): 297-304
doi: 10.11862/CJIC.2016.032
Abstract:
One novel nitronyl nitroxide radical and its three mononuclear tri-spin compounds Ln (hfac)3(NIT-Ph-4-OCHCH3CH3)2 (Ln=Gd (1), Tb (2), Dy (3); hfac=hexafluoroacetylacetonate; NIT-Ph-4-OCHCH3CH3=2-(4-isopropoxyphenyl)-4, 4, 5, 5-tetramethyl-imidazoline-1-oxyl-3-oxide) have been successfully prepared and characterized. Single crystal X-ray crystallographic analyses reveal that complexes 1, 2, and 3 shows similar radical-Ln (Ⅲ)-radical structures, which ar composed of one Ln (hfac)3 units and two NIT-Ph-4-OCHCH3CH3 radicals. Magnetic studies reveal that ferromagnetic interactions (between intramolecular Ln and radical) and antiferromagnetic interactions (between the intramolecular radicals) are coexist in these complexes. CCDC: 985443, 1; 1043098, 2; 985444, 3.
One novel nitronyl nitroxide radical and its three mononuclear tri-spin compounds Ln (hfac)3(NIT-Ph-4-OCHCH3CH3)2 (Ln=Gd (1), Tb (2), Dy (3); hfac=hexafluoroacetylacetonate; NIT-Ph-4-OCHCH3CH3=2-(4-isopropoxyphenyl)-4, 4, 5, 5-tetramethyl-imidazoline-1-oxyl-3-oxide) have been successfully prepared and characterized. Single crystal X-ray crystallographic analyses reveal that complexes 1, 2, and 3 shows similar radical-Ln (Ⅲ)-radical structures, which ar composed of one Ln (hfac)3 units and two NIT-Ph-4-OCHCH3CH3 radicals. Magnetic studies reveal that ferromagnetic interactions (between intramolecular Ln and radical) and antiferromagnetic interactions (between the intramolecular radicals) are coexist in these complexes. CCDC: 985443, 1; 1043098, 2; 985444, 3.
2016, 32(2): 305-312
doi: 10.11862/CJIC.2015.042
Abstract:
A new magnesium borate mineral, Mg[B6O7(OH)6]·5H2O was synthesized via dilution method from boron-bearing Na-K-Mg-Cl-SO4 salt lakes. The crystal structure of the new phase was solved and refined using X-ray powder diffraction data and characterized with FTIR and Raman. Its asymmetric unit consists of one Mg atom, one B6O7(OH)6 cluster and five H2O molecules. The Mg atom is 6-coordinated with six O atoms to form a MgO6 octahedron. Thermal gravimetry (TG/DSC) was used to investigate the thermal behavior of the new compound. During the high temperature decomposition process the dehydrated product MgB4O7 formed. The optical absorption characteristic of this new mineral was investigated by UV-Vis spectrometer and its energy gap Eg is about 4.44 eV.
A new magnesium borate mineral, Mg[B6O7(OH)6]·5H2O was synthesized via dilution method from boron-bearing Na-K-Mg-Cl-SO4 salt lakes. The crystal structure of the new phase was solved and refined using X-ray powder diffraction data and characterized with FTIR and Raman. Its asymmetric unit consists of one Mg atom, one B6O7(OH)6 cluster and five H2O molecules. The Mg atom is 6-coordinated with six O atoms to form a MgO6 octahedron. Thermal gravimetry (TG/DSC) was used to investigate the thermal behavior of the new compound. During the high temperature decomposition process the dehydrated product MgB4O7 formed. The optical absorption characteristic of this new mineral was investigated by UV-Vis spectrometer and its energy gap Eg is about 4.44 eV.
2016, 32(2): 320-326
doi: 10.11862/CJIC.2016.027
Abstract:
Two new transition metal coordination polymers, {[Cu (Hmptc)(H2O)]·2H2O}n (1) and {Cd (Hmptc)(H2O)}n (2), were successfully constructed from transition metal salts with 6-methyl-2, 3, 5-pyridinetricarboxylic acid (H3mptc). Complex 1 exhibits a 2D coordination network, in which rectangle channels are shown to exist. In complex 2, Cd (Ⅱ) centers are linked by Hmptc2- ligands into 2D grid-like layers, which are further linked by hydrogen bonding interactions to form a 3D supramolecular network. In addition, complex 2 exhibits blue/green luminescence in the solid state at room temperature. CCDC: 906071, 1; 906072, 2.
Two new transition metal coordination polymers, {[Cu (Hmptc)(H2O)]·2H2O}n (1) and {Cd (Hmptc)(H2O)}n (2), were successfully constructed from transition metal salts with 6-methyl-2, 3, 5-pyridinetricarboxylic acid (H3mptc). Complex 1 exhibits a 2D coordination network, in which rectangle channels are shown to exist. In complex 2, Cd (Ⅱ) centers are linked by Hmptc2- ligands into 2D grid-like layers, which are further linked by hydrogen bonding interactions to form a 3D supramolecular network. In addition, complex 2 exhibits blue/green luminescence in the solid state at room temperature. CCDC: 906071, 1; 906072, 2.
2016, 32(2): 327-335
doi: 10.11862/CJIC.2016.034
Abstract:
Two new Cu (Ⅱ) complexes [Cu (L1)2](1) (HL1=1-(3-((2-hydroxybenzylidene) amino) phenyl) ethanone O-benzyl oxime) and [Cu (L2)2] (2) (HL2 =1-(3-((2-Hydroxy-naphthalen-1-ylmethylene)-amino)-phenyl)-ethanone oxime) have been synthesized and characterized by elemental analyses, IR spectra, UV-Vis spectra, fluorescence measurement and X-ray single crystal diffraction method. X-ray crystallographic analyses have indicated that complexes 1 and 2 have the similar structure, consisting of one Cu (Ⅱ) ion, two ligand units. In the complexes, the Cu (Ⅱ) ion lying on an inversion centre, is four-coordinated in a trans-CuN2O2 square-planar geometry by two hydroxy O and two imine N atoms from two symmetry-related N, O-bidentate Schiff base ligands. The supramolecular structures of the two complexes 1 and 2 are also similar two-dimensional supramolecular structure linking by different intermolecular interaction. Complex 1 forms an infinite two-dimensional supramolecular structure by two π…π interaction, while that of complex 2 by intermolecular O-H…N and C-H…π hydrogen bond interactions. The fluorescence property of complex 1 and substituent effects of the two complexes are discussed. CCDC: 1003363, 1; 1043506, 2.
Two new Cu (Ⅱ) complexes [Cu (L1)2](1) (HL1=1-(3-((2-hydroxybenzylidene) amino) phenyl) ethanone O-benzyl oxime) and [Cu (L2)2] (2) (HL2 =1-(3-((2-Hydroxy-naphthalen-1-ylmethylene)-amino)-phenyl)-ethanone oxime) have been synthesized and characterized by elemental analyses, IR spectra, UV-Vis spectra, fluorescence measurement and X-ray single crystal diffraction method. X-ray crystallographic analyses have indicated that complexes 1 and 2 have the similar structure, consisting of one Cu (Ⅱ) ion, two ligand units. In the complexes, the Cu (Ⅱ) ion lying on an inversion centre, is four-coordinated in a trans-CuN2O2 square-planar geometry by two hydroxy O and two imine N atoms from two symmetry-related N, O-bidentate Schiff base ligands. The supramolecular structures of the two complexes 1 and 2 are also similar two-dimensional supramolecular structure linking by different intermolecular interaction. Complex 1 forms an infinite two-dimensional supramolecular structure by two π…π interaction, while that of complex 2 by intermolecular O-H…N and C-H…π hydrogen bond interactions. The fluorescence property of complex 1 and substituent effects of the two complexes are discussed. CCDC: 1003363, 1; 1043506, 2.
2016, 32(2): 351-359
doi: 10.11862/CJIC.2016.044
Abstract:
A new infrared spectroscopic measurement of interstitial oxygen and substitutional carbon in silicon wafers at room temperature by Multiple Transmission-Reflection Infrared Spectroscopy (MTR-IR) has been established. The superiority of MTR-IR to conventional IR has been analyzed first in principle by theoretical calculation and then verified by practical measurements of single crystalline silicon samples. The advantages of MTR-IR over conventional IR with a single normal incidence are: (1) The absorption bands of interstitial oxygen at 1 107 cm-1 and substitutional carbon at 605 cm-1 can be enhanced linearly with the simplified transmission times (N) between 6 and 12, which consequently extends the detection limit of oxygen and carbon at least one order of magnitude lower. (2) The strength of interference fringes can be decreased for a 0.2 mm thin silicon slice by 23 times as that from the single normal incidence and 11 times as that from the Brewster angle transmission respectively. (3) Not like the conventional IR method, only collecting data from one sampling point at each measurement, MTR-IR collects data from multiple sampling points in a longer sample for one measurement. Overall, both theoretical calculations and experimental results demonstrate the high sensitivity, reliability, and reproducibility of the MTR-IR spectroscopy on the measurement of impurities of interstitial oxygen and substitutional carbon of single crystalline silicon.
A new infrared spectroscopic measurement of interstitial oxygen and substitutional carbon in silicon wafers at room temperature by Multiple Transmission-Reflection Infrared Spectroscopy (MTR-IR) has been established. The superiority of MTR-IR to conventional IR has been analyzed first in principle by theoretical calculation and then verified by practical measurements of single crystalline silicon samples. The advantages of MTR-IR over conventional IR with a single normal incidence are: (1) The absorption bands of interstitial oxygen at 1 107 cm-1 and substitutional carbon at 605 cm-1 can be enhanced linearly with the simplified transmission times (N) between 6 and 12, which consequently extends the detection limit of oxygen and carbon at least one order of magnitude lower. (2) The strength of interference fringes can be decreased for a 0.2 mm thin silicon slice by 23 times as that from the single normal incidence and 11 times as that from the Brewster angle transmission respectively. (3) Not like the conventional IR method, only collecting data from one sampling point at each measurement, MTR-IR collects data from multiple sampling points in a longer sample for one measurement. Overall, both theoretical calculations and experimental results demonstrate the high sensitivity, reliability, and reproducibility of the MTR-IR spectroscopy on the measurement of impurities of interstitial oxygen and substitutional carbon of single crystalline silicon.
2016, 32(2): 369-376
doi: 10.11862/CJIC.2016.040
Abstract:
An aroylhydrazone compound, N′-(3-bromo-5-chloro-2-hydroxybenzylidene)-3-hydroxyl-4-methoxyben-zohydrazide (H2L), was prepared and characterized by elemental analysis, IR, UV, HRMS, 1H NMR and 13C NMR spectrum. Reaction of H2L, maltol (3-hydroxy-2-methyl-4-pyrone) and VO (acac)2 in methanol afforded a maltolato-coordinated oxovanadium (Ⅴ) complex, [VO (mat) L]·MeOH. The complex was characterized by elemental analysis, IR and UV spectra. Thermal analysis was also performed. Structures of H2L and the complex were further confirmed by single crystal X-ray diffraction. Insulin-mimetic tests on C2C12 muscle cells indicate that the complex significantly stimulated cell glucose utilization with cytotoxicity at 0.07 g·L-1. CCDC: 1437202, H2L; 1437201, the complex.
An aroylhydrazone compound, N′-(3-bromo-5-chloro-2-hydroxybenzylidene)-3-hydroxyl-4-methoxyben-zohydrazide (H2L), was prepared and characterized by elemental analysis, IR, UV, HRMS, 1H NMR and 13C NMR spectrum. Reaction of H2L, maltol (3-hydroxy-2-methyl-4-pyrone) and VO (acac)2 in methanol afforded a maltolato-coordinated oxovanadium (Ⅴ) complex, [VO (mat) L]·MeOH. The complex was characterized by elemental analysis, IR and UV spectra. Thermal analysis was also performed. Structures of H2L and the complex were further confirmed by single crystal X-ray diffraction. Insulin-mimetic tests on C2C12 muscle cells indicate that the complex significantly stimulated cell glucose utilization with cytotoxicity at 0.07 g·L-1. CCDC: 1437202, H2L; 1437201, the complex.
